CN104003705A - Method for sintering multiferroic bismuth ferrite-based electronic functional ceramics - Google Patents
Method for sintering multiferroic bismuth ferrite-based electronic functional ceramics Download PDFInfo
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Abstract
The invention provides a method for sintering multiferroic bismuth ferrite-based electronic functional ceramics, which comprises the following steps: mixing Fe2O3, Bi2O3, BaCO3, TiO2, and MnO2 powder according to a mole ratio of 34-40:34-40:20-32:20-32:0.4, performing ball milling, drying, tabletting, and presintering in a sintering furnace; crushing the presintered ceramic chips, performing ball milling to obtain powder, and performing solid-phase sintering; crushing the ceramic chip after solid-phase sintering, and performing ball milling and spark plasma sintering. The multiferroic bismuth ferrite-based electronic functional ceramics prepared by the invention have very good phase structure and compactness, and have significantly improved ferroelectricity and piezoelectricity. The process is simple; the spark plasma sintering temperature is low; and the production is safer.
Description
Technical field
The invention belongs to function ceramics field, be specifically related to a kind of method of sintering multiferroic ferrous acid bismuthino electric function ceramic.
Background technology
The stupalith that the functions such as electric function ceramic refers to the detection of electricity, magnetic, light, sound, heat, power, chemistry and the information such as biological, changes, coupling, transmission and storage are principal character, mainly comprises piezoelectricity, dielectric, superconduction and magnetic ceramics etc.Electronic ceramics occupies very consequence in miniaturization and portable type electronic product, and countries in the world components and parts manufacturing enterprise all researchs and develops dropping into huge fund aspect the product innovation of electronic ceramics and components and parts thereof, new technology, novel process, novel material, new installation.There are every year a large amount of new function stupaliths and components and parts to come out.
Why unique properties of electric function ceramic, this mainly relies on the chemical constitution of material, also with prepare synthetic technological condition and material microstructure and have close associated.The preparation of electric function ceramic is roughly in two steps: the sintering of the preparation of powder and pottery sheet.Conventionally the state classification that the preparation method of ceramic powder presses material, mainly contains solid phase method and liquid phase method.
Solid phase method is the traditional method of preparing electric function ceramic.Its basic technology is that raw material is prepared by required stoichiometric ratio, then, through ball milling blending dispersion, pre-burning, obtains ceramic powder.The advantage of this method is technology maturation, and technique is simple, with low cost, and therefore current industrial production still adopts this method in a large number.But also there are many inevitable shortcomings in this method: in (1) raw material, each component is difficult to be mixed into desirable uniform state; (2) calcining temperature is high; (3) high-temperature lower part divides raw material volatile, thereby is difficult to obtain the sintered compact in strict conformity with stoichiometric ratio; (4) in whole technological process, easily mix, can not get the powder that purity is high, will finally affect the performance of material.
The ultimate principle of liquid phase method is to select one or more soluble metallic salts, the according to target chemical composition wiring solution-forming of material, make each element be lewis' acid state, select again a kind of suitable precipitation agent or select the means such as evaporation, distillation, hydrolysis, by metal ion precipitation from homogeneous solution or crystallize out, gained precipitation or crystallisate can make super-fine powder through dehydration or thermal degradation.Each component is mixed on molecular level, and material is uniformly dispersed, and preparation temperature has substantial degradation than traditional method, is easy to doping.But, due to the solvability difference of different metal salt in solution, can affect to a certain extent the chemistry of stupalith and the homogeneity of structure, and be difficult to avoid completely the generation of side reaction.
And the sintering method of pottery sheet generally can be divided into: normal sintering, reaction sintering, hot pressed sintering etc.Normal sintering is the sintering method the most often adopting during current stupalith is produced, but the pottery sheet relative density of sintering is lower, can not fully meet the demand of premium quality product; Reaction sintering is only confined to a small amount of a few individual system: silicon nitride, silicon oxynitride, silicon carbide etc., and it can make complex-shaped accurate in size goods, technique is simple, economical, be applicable to producing in enormous quantities, but sintered blank density is low, and material mechanical performance is not high; Hot pressed sintering adopts special thermocompressor, at high temperature single-phase or two-phase has been exerted pressure, can obtain almost imporous goods, but can only manufacture the goods of simple shape, after hot pressed sintering, microtexture has anisotropy simultaneously, causes use properties also to have anisotropy, limit its use range, in addition,, because hardness is high, the following process of hot-pressed product is difficulty especially.
Above-mentioned sintering method has the shortcoming that relative density is lower, dephasign is more in the time of preparation multiferroic stupalith, and the performance of sintered sample is difficult to be guaranteed.Therefore, seek novel sintered technology and become study hotspot.
Discharge plasma sintering (Spark Plasma Sintering, SPS), claim again plasma activated sintering (Plasma Activated Sintering, or plasma assisted sintering (Plasma Assisted Sintering PAS), PAS), be a kind of novel Fast Sintering technology that development in recent years is got up.Discharge plasma sintering technique melts plasma activation, hot pressing, resistive heating is integrated, there is heat-up rate fast, sintering time is short, cooling rapid, impressed pressure and sintering atmosphere are controlled, the features such as energy-conserving and environment-protective, can be widely used in magneticsubstance, function-graded material, nano ceramics, the sintering of the series of new materials such as fiber reinforced ceramic and intermetallic matrix material, and in nano material, in the preparation of matrix material etc., show great superiority, it is a sintering new technology that has important use value and extensive prospect, also be one and there is huge economic value, the research field of technological value and wide application prospect.
Summary of the invention
For these reasons, the present invention adopts solid phase method to prepare ceramic powder the method in conjunction with discharge plasma sintering, and acquisition relative density is high, well-crystallized's multiferroic ferrous acid bismuthino electric function ceramic.
A kind of method that the invention provides sintering multiferroic ferrous acid bismuthino electric function ceramic, comprises the steps:
(1) presintering
By Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2and MnO
2powder is that the ratio of 34 ~ 40:34 ~ 40:20 ~ 32:20 ~ 32:0.4 is mixed and ball milling was dried after 10 ~ 20 hours in molar ratio, compressing tablet, the columnar block pressing is positioned over to sintering in sintering oven, and presintering naturally cooling after 3 ~ 6 hours at 800 ~ 880 DEG C, obtains the ceramic plate of presintering;
(2) solid state sintering
The ceramic plate of the presintering that step (1) is made is through pulverizing and after ball milling is powder, compressing tablet, is placed in sintering oven sintering by the columnar block pressing, and solid state sintering sintering naturally cooling after 2 ~ 3 hours at 900 ~ 960 DEG C obtains the ceramic plate of solid state sintering;
(3) discharge plasma sintering
Open the water coolant of sintering oven, the ceramic plate of the solid state sintering that step (2) is made is put into sintering cavity after pulverizing, two ends apply the axle pressure of 30 ~ 50MPa, vacuumize, agglomerating chamber's air pressure starts heating while being the vacuum tightness of 80Pa, heat-up rate is 50 ~ 100 DEG C/min, in the time that temperature is increased to 630 ~ 660 DEG C, start discharge plasma sintering and keep 5 ~ 10 minutes, sintering is complete, stop heating removal pressure, cool to room temperature with the furnace, obtain multiferroic ferrous acid bismuthino electric function ceramic.
In step (1), Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2and MnO
2the mol ratio of powder is 39:39:22:22:0.4.
Described Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2and MnO
2purity all more than 99.9%.
The method of a kind of sintering multiferroic ferrous acid bismuthino electric function ceramic provided by the invention, by traditional solid state sintering is combined with discharge plasma sintering, annealing in a vacuum again, the multiferroic ferrous acid bismuthino electric function ceramic preparing has good phase constitution and compactness, ferroelectricity, piezoelectricity are all significantly improved, and technique is simple, discharge plasma sintering temperature is low, produces safer.
Brief description of the drawings
Fig. 1 is the profile scanning Electronic Speculum figure of multiferroic ferrous acid bismuthino electric function ceramic in embodiment 1, and wherein illustration is the enlarged view of peak (111);
Fig. 2 is the X ray diffracting spectrum of multiferroic ferrous acid bismuthino electric function ceramic in embodiment 1;
Fig. 3 is the residual polarization graphic representation of multiferroic ferrous acid bismuthino electric function ceramic in embodiment 1, and wherein curve 1 is the lower 500 DEG C of annealing of the vacuum condition residual polarization graphic representation of 1 hour, and curve 2 is 600 DEG C of annealing residual polarization graphic representation of 1 hour in oxygen atmosphere;
Fig. 4 is multiferroic ferrous acid bismuthino electric function ceramic 600 DEG C of annealing dielectric properties figure of 1 hour in air in embodiment 1;
Fig. 5 is multiferroic ferrous acid bismuthino electric function ceramic 500 DEG C of annealing dielectric properties figure of 1 hour in a vacuum in embodiment 1.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples, and described method is ordinary method if no special instructions.The Fe that the present invention uses
2o
3purity is 99.99%, is buied by Johnson-Matthey company; Bi
2o
3purity is 99.9%, is buied by Kishida company; BaCO
3purity is 99.99%, is buied by Kanto Chemical company; TiO
2purity is 99.9%, is buied by Aldrich Chemical company; MnO
2purity is 99.99%, is buied by Aldrich Chemical company.The relative density the present invention relates to is the ratio of actual density and Theoretical Calculation density.
Embodiment 1
By Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2and MnO
2for the ratio of 39:39:22:22:0.4 is mixed, also ball milling is after 15 hours in molar ratio, and dry, compressing tablet, is positioned over sintering in sintering oven by the columnar block pressing, presintering 5 hours at 850 DEG C, naturally cooling; The ceramic plate of presintering is through pulverizing and after ball milling is powder, compressing tablet, is placed in sintering oven sintering by the columnar block pressing, and solid state sintering sintering naturally cooling after 2 hours at 950 DEG C obtains the ceramic plate of solid state sintering; Open the water coolant of sintering oven, after the ceramic plate of the solid state sintering making is pulverized, put into sintering cavity, two ends apply the axle pressure of 50MPa, vacuumize, agglomerating chamber's air pressure starts heating while being the vacuum tightness of 80Pa, heat-up rate is 100 DEG C/min, starts discharge plasma sintering and keep 5 minutes in the time that temperature is increased to 650 DEG C, and sintering is complete, stop heating removal pressure, cool to room temperature with the furnace, obtain multiferroic ferrous acid bismuthino electric function ceramic, relative density is 96%.
With the each stage phase composite of X-ray diffractometer (RINT 2000, Rigaku) detection sample sintering, as shown in Figure 1, be typical tripartite's phase structure, there is no the diffraction peak of other dephasign.As shown in Figure 2, ceramic particle granularity is 5 ~ 9 μ m to the profile scanning Electronic Speculum figure of gained multiferroic ferrous acid bismuthino electric function ceramic, dense structure, well-crystallized.
Embodiment 2
By Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2and MnO
2for the ratio of 34:34:32:32:0.4 is mixed, also ball milling is after 20 hours in molar ratio, and dry, compressing tablet, is positioned over sintering in sintering oven by the columnar block pressing, presintering 6 hours at 880 DEG C, naturally cooling; The ceramic plate of presintering is through pulverizing and after ball milling is powder, compressing tablet, is placed in sintering oven sintering by the columnar block pressing, and solid state sintering sintering naturally cooling after 3 hours at 960 DEG C obtains the ceramic plate of solid state sintering; Open the water coolant of sintering oven, after the ceramic plate of the solid state sintering making is pulverized, put into sintering cavity, two ends apply the axle pressure of 50MPa, vacuumize, agglomerating chamber's air pressure starts heating while being the vacuum tightness of 80Pa, heat-up rate is 100 DEG C/min, starts discharge plasma sintering and keep 10 minutes in the time that temperature is increased to 660 DEG C, and sintering is complete, stop heating removal pressure, cool to room temperature with the furnace, obtain multiferroic ferrous acid bismuthino electric function ceramic, relative density is 92%.
Embodiment 3
By Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2and MnO
2for the ratio of 40:40:20:20:0.4 is mixed, also ball milling is after 10 hours in molar ratio, and dry, compressing tablet, is positioned over sintering in sintering oven by the columnar block pressing, presintering 3 hours at 800 DEG C, naturally cooling; The ceramic plate of presintering is through pulverizing and after ball milling is powder, compressing tablet, is placed in sintering oven sintering by the columnar block pressing, and solid state sintering sintering naturally cooling after 2 hours at 900 DEG C obtains the ceramic plate of solid state sintering; Open the water coolant of sintering oven, after the ceramic plate of the solid state sintering making is pulverized, put into sintering cavity, two ends apply the axle pressure of 30MPa, vacuumize, agglomerating chamber's air pressure starts heating while being the vacuum tightness of 80Pa, heat-up rate is 50 DEG C/min, starts discharge plasma sintering and keep 8 minutes in the time that temperature is increased to 630 DEG C, and sintering is complete, stop heating removal pressure, cool to room temperature with the furnace, obtain multiferroic ferrous acid bismuthino electric function ceramic, relative density is 93%.
Embodiment 4
The multiferroic ferrous acid bismuthino electric function ceramic that embodiment 1 is made carries out performance test.
Adopt retort furnace (L22-I/RZQ) to carry out oxygen annealing to it, the vacuum withdraw device (GP-2A) that adopts infrared induction process furnace (Image Furnace) to obtain good temperature control condition and ULVAC company obtains the vacuum annealing environment that barometric point is 1Pa; Sample resistivity under Different Heat Treatment Conditions is tested with HP4339A-HP16339A type Insulation Resistance Tester.As shown in Figure 3, under vacuum condition, the remnant polarization of the sample after annealing reaches 59.5 μ C/cm
2, compared with 18.5 μ C/cm of the sample of anneal in oxygen
2being significantly improved, is that in such stupalith of having reported at present, remnant polarization is the highest.
Use HP4284 and HP4285 analyser to measure its dielectric characteristics, test frequency is respectively 75kHz, 120kHz, 300kHz, 1MHz, 3MHz and 10MHz, as shown in Figure 4, the dielectric frequency dispersal degree of the sample of annealing in process oxygen is higher, loss is also larger, as shown in Figure 5, the ceramic dielectric loss of annealing under vacuum condition is less, and dielectric frequency dispersal degree decreases.
Adopt the piezoelectricity tester of Acoustical Inst., Chinese Academy of Sciences to carry out piezo-electric modulus
d 33measurement (ZJ-6B), record piezo-electric modulus
d 33=39.6pC/N, this material prepared by traditional solid phase method
d 33=20pC/N, in comparison, between the mechanical energy of the multiferroic ferrous acid bismuthino electric function ceramic that the present invention makes and electric energy, efficiency of conversion is higher.
Claims (3)
1. a method for sintering multiferroic ferrous acid bismuthino electric function ceramic, is characterized in that, comprises the steps:
(1) presintering
By Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2and MnO
2powder is that the ratio of 34 ~ 40:34 ~ 40:20 ~ 32:20 ~ 32:0.4 is mixed and ball milling was dried after 10 ~ 20 hours in molar ratio, compressing tablet, the columnar block pressing is positioned over to sintering in sintering oven, and presintering naturally cooling after 3 ~ 6 hours at 800 ~ 880 DEG C, obtains the ceramic plate of presintering;
(2) solid state sintering
The ceramic plate of the presintering that step (1) is made is through pulverizing and after ball milling is powder, compressing tablet, is placed in sintering oven sintering by the columnar block pressing, and solid state sintering sintering naturally cooling after 2 ~ 3 hours at 900 ~ 960 DEG C obtains the ceramic plate of solid state sintering;
(3) discharge plasma sintering
Open the water coolant of sintering oven, the ceramic plate of the solid state sintering that step (2) is made is put into sintering cavity after pulverizing, two ends apply the axle pressure of 30 ~ 50MPa, vacuumize, agglomerating chamber's air pressure starts heating while being the vacuum tightness of 80Pa, heat-up rate is 50 ~ 100 DEG C/min, in the time that temperature is increased to 630 ~ 660 DEG C, start discharge plasma sintering and keep 5 ~ 10 minutes, sintering is complete, stop heating removal pressure, cool to room temperature with the furnace, obtain multiferroic ferrous acid bismuthino electric function ceramic.
2. the method for a kind of sintering multiferroic ferrous acid bismuthino electric function ceramic according to claim 1, is characterized in that, in step (1), and Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2and MnO
2the mol ratio of powder is 39:39:22:22:0.4.
3. the method for a kind of sintering multiferroic ferrous acid bismuthino electric function ceramic according to claim 1, is characterized in that described Fe
2o
3, Bi
2o
3, BaCO
3, TiO
2and MnO
2purity all more than 99.9%.
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Cited By (3)
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| CN106927809A (en) * | 2015-12-30 | 2017-07-07 | 中国科学院上海硅酸盐研究所 | A kind of high polarization intensity bismuth ferrite ceramic material and preparation method thereof |
| CN107285766A (en) * | 2017-04-28 | 2017-10-24 | 武汉理工大学 | A kind of high electric field induced strain lead-free ceramicses fiber and preparation method thereof |
| CN109354487A (en) * | 2018-10-11 | 2019-02-19 | 江西科技学院 | A kind of bismuth ferrite base nano ceramic and preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927809A (en) * | 2015-12-30 | 2017-07-07 | 中国科学院上海硅酸盐研究所 | A kind of high polarization intensity bismuth ferrite ceramic material and preparation method thereof |
| CN106927809B (en) * | 2015-12-30 | 2020-11-10 | 中国科学院上海硅酸盐研究所 | High-polarization-strength bismuth ferrite ceramic material and preparation method thereof |
| CN107285766A (en) * | 2017-04-28 | 2017-10-24 | 武汉理工大学 | A kind of high electric field induced strain lead-free ceramicses fiber and preparation method thereof |
| CN107285766B (en) * | 2017-04-28 | 2020-05-05 | 武汉理工大学 | High-electrostriction lead-free ceramic fiber and preparation method thereof |
| CN109354487A (en) * | 2018-10-11 | 2019-02-19 | 江西科技学院 | A kind of bismuth ferrite base nano ceramic and preparation method |
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Application publication date: 20140827 |